CN105642320A - Samarium-doped KMgF3 perovskite type visible light response catalyst and preparation method thereof - Google Patents
Samarium-doped KMgF3 perovskite type visible light response catalyst and preparation method thereof Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 47
- 230000004298 light response Effects 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 229910052772 Samarium Inorganic materials 0.000 claims abstract description 35
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 claims abstract description 35
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- 238000005119 centrifugation Methods 0.000 claims description 15
- MFUVDXOKPBAHMC-UHFFFAOYSA-N magnesium;dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MFUVDXOKPBAHMC-UHFFFAOYSA-N 0.000 claims description 14
- 239000004530 micro-emulsion Substances 0.000 claims description 14
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 11
- BWDBEAQIHAEVLV-UHFFFAOYSA-N 6-methylheptan-1-ol Chemical compound CC(C)CCCCCO BWDBEAQIHAEVLV-UHFFFAOYSA-N 0.000 claims description 8
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 7
- 150000002500 ions Chemical class 0.000 claims description 7
- 238000001354 calcination Methods 0.000 claims description 6
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 6
- 238000013019 agitation Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- 239000004323 potassium nitrate Substances 0.000 claims description 4
- 235000010333 potassium nitrate Nutrition 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- -1 hydrate samarium potassium nitrate Chemical compound 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000011941 photocatalyst Substances 0.000 abstract description 13
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 abstract description 13
- 229940043267 rhodamine b Drugs 0.000 abstract description 13
- 230000001699 photocatalysis Effects 0.000 abstract description 7
- 230000015556 catabolic process Effects 0.000 abstract description 5
- 238000006731 degradation reaction Methods 0.000 abstract description 5
- 230000000593 degrading effect Effects 0.000 abstract description 2
- 238000000593 microemulsion method Methods 0.000 abstract description 2
- 239000002351 wastewater Substances 0.000 abstract description 2
- 239000002245 particle Substances 0.000 abstract 2
- 230000010757 Reduction Activity Effects 0.000 abstract 1
- 238000005215 recombination Methods 0.000 abstract 1
- 230000006798 recombination Effects 0.000 abstract 1
- 239000010936 titanium Substances 0.000 description 20
- 238000002474 experimental method Methods 0.000 description 9
- 238000003756 stirring Methods 0.000 description 9
- 229910002651 NO3 Inorganic materials 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- YIWUKEYIRIRTPP-UHFFFAOYSA-N 2-ethylhexanol Substances CCCCC(CC)CO YIWUKEYIRIRTPP-UHFFFAOYSA-N 0.000 description 4
- 238000002835 absorbance Methods 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- 238000010531 catalytic reduction reaction Methods 0.000 description 4
- 230000010355 oscillation Effects 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 239000006228 supernatant Substances 0.000 description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 3
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical compound [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 description 3
- 239000000975 dye Substances 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- IPFZYNPDAIWERQ-UHFFFAOYSA-N samarium;hydrate Chemical compound O.[Sm] IPFZYNPDAIWERQ-UHFFFAOYSA-N 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033558 biomineral tissue development Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 239000007857 degradation product Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- NMGYKLMMQCTUGI-UHFFFAOYSA-J diazanium;titanium(4+);hexafluoride Chemical compound [NH4+].[NH4+].[F-].[F-].[F-].[F-].[F-].[F-].[Ti+4] NMGYKLMMQCTUGI-UHFFFAOYSA-J 0.000 description 1
- 239000010919 dye waste Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000003836 solid-state method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
- B01J27/138—Halogens; Compounds thereof with alkaline earth metals, magnesium, beryllium, zinc, cadmium or mercury
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a samarium-doped KMgF3 perovskite type visible light response catalyst and further discloses a preparation method of the samarium-doped KMgF3 perovskite type visible light response catalyst. The samarium-doped KMgF3 perovskite type visible light response catalyst is high in visible light utilization rate and has high photocatalytic activity under visible light, samarium doping can effectively prevent recombination of electrons and holes, and the degradation rate of dye molecules, especially rhodamine B is greatly raised. The preparation method includes the steps that firstly, nanometer particles of the samarium-doped KMgF3 perovskite type visible light response catalyst are prepared through a micro-emulsion method, then the nanometer particles are sintered in a tube furnace to be crystallized, compared with a pure KMgF3 perovskite type photocatalyst, the photocatalytic reduction activity on the dye molecules of the catalyst under visible light is greatly improved, and thus the visible light response catalyst can be used for degrading dye wastewater.
Description
Technical field
The present invention relates to a kind of samarium doping KMgF3Ca-Ti ore type visible light response catalyst, further relates to above-mentioned samarium doping KMgF3The preparation method of Ca-Ti ore type visible light response catalyst, belongs to photocatalyst field.
Background technology
In recent years, along with China's rapid development of economy, commercial scale expanding day, the process of industrial wastewater increasingly causes society's attention. Wherein, waste water from dyestuff is because of its complicated component, the feature such as colourity is high, organic concentration high, toxicity is big, and environmental pollution is very big, especially the physiological health of the mankind and other biological is caused serious threat. Therefore, research and development utility model Treatment process is to the protection of ecological environment, human life's health, the great theory of social sustainable development and practical significance.
In numerous dye wastewater treatment technologies, photocatalysis technology is nontoxic with it, chemically stable, reaction condition gentle, the advantages such as thorough, non-secondary pollution of degrading become domestic and international academia study hotspot. In numerous photocatalysts, TiO2It is the photocatalyst of current most study, but its energy gap relatively big (3.2eV), Solar use is inefficient, only about 5.4%, limit its extensive use. Perovskite type photocatalyst, because it has perovskite crystal structure, stable chemical performance, it is seen that light utilization efficiency is high, is just subject to people's attention gradually.
Wang Li et al. is at " silicate circular ", 2008,27 (2): 394-397 " nanometer KCaF delivered3The research of preparation and photocatalytic activity " in a literary composition, adopt high temperature solid-state method and solvent structure nano-perovskite type composite fluoride KCaF3Powder. But still have the disadvantage that target degradation product mineralization rate is low, visible ray utilization rate is low.
Chinese patent CN102319576A, a kind of fluoride photocatalytic material and preparation method thereof, this patent bismuth nitrate, ammonium titanium fluoride have synthesized a kind of fluoride stratiform perovskite type photocatalyst under hydrothermal conditions. But still have the disadvantage that under visible light almost without photocatalytic activity.
Therefore the exploitation of a kind of visible light response catalyst under visible light with highlight catalytic active is necessary.
Summary of the invention
The technical problem to be solved is to provide the samarium doping KMgF under a kind of visible ray with highlight catalytic active3Ca-Ti ore type visible light response catalyst, this catalyst greatly improves its utilization rate to visible ray after samarium doped, thus making it have high visible light activity.
The present invention also to solve the technical problem that and be to provide the samarium doping KMgF under above-mentioned visible ray with highlight catalytic active3The preparation method of Ca-Ti ore type visible light response catalyst.
For solving above-mentioned technical problem, the technical solution adopted in the present invention is:
A kind of samarium doping KMgF3Ca-Ti ore type visible light response catalyst, for every 1molKMgF3, Sm3+The doping of ion is 0.01��0.03mol, Sm3+Ion doping is in B bit element Mg2+On ion.
Above-mentioned samarium doping KMgF3The preparation method of Ca-Ti ore type visible light response catalyst, comprises the steps:
Step 1, adds a certain amount of cetyl trimethylammonium bromide in isooctanol, is configured to solution A after mixing; A certain amount of potassium nitrate, magnesium nitrate hexahydrate and six nitric hydrate samariums are added to the water, are configured to solution B; A certain amount of ammonium fluoride is added to the water, is configured to solution C; Under constant agitation, successively solution B and solution C are added dropwise in solution A, form the microemulsion of homogeneous transparent continuously stirred a period of time;
Step 2, the microemulsion centrifugation that step 1 is obtained, undertaken the precipitation after centrifugal washing, dried;
Step 3, calcines the product of step 2 in nitrogen atmosphere, namely obtains samarium doping KMgF after calcining cooling3Ca-Ti ore type visible light response catalyst.
Wherein, in step 1, in solution A, the addition mass ratio of described cetyl trimethylammonium bromide and isooctanol is 1: 6.
Wherein, in step 1, in described microemulsion, the addition mol ratio of potassium nitrate, magnesium nitrate hexahydrate, six nitric hydrate samarium potassium nitrate and ammonium fluoride is 1: 1: 0.01��0.03: 3.
Wherein, in step 2, the speed of described centrifugation is 4000r/min, and the time is 15min; The cleaning mixture that described washing adopts is methanol.
Wherein, in step 3, the temperature of described calcining is 400 DEG C, and described calcination process is to be risen to 400 DEG C by room temperature, and its heating rate is: 10 DEG C/min
Samarium doping KMgF of the present invention3The preparation principle of Ca-Ti ore type visible light response catalyst: the present invention is first with microemulsion method, with cetyl trimethylammonium bromide (CTAB) for surfactant, isooctanol (2-EH) is oil phase, the solion of reactant is aqueous phase, and three mixes with certain proportion, forms microemulsion, in this microemulsion system, water core constantly collides so that it is in reactant ion swap, formed final catalyst nanoparticle; The nanoparticle centrifugation of final catalyst that will obtain again, and wash for several times with methanol, dry, obtain catalyst powder; Last at 400 DEG C, nitrogen atmosphere is calcined so that it is crystallization, finally give samarium doping KMgF3Ca-Ti ore type visible light response catalyst.
Beneficial effect: compared to prior art, the samarium doping KMgF of the present invention3Ca-Ti ore type visible light response catalyst, at visible light wave range, has high utilization rate, has high photocatalytic activity under visible light; Samarium doping can effectively stop the compound in electronics and hole, and degradation rate to dye molecule, particularly rhodamine B is substantially improved, the samarium doping KMgF of the present invention3Ca-Ti ore type visible light response catalyst, the under visible light degradation rate to rhodamine B, can reach 90% in 1h, and therefore the visible light response catalyst of the present invention can be used for degradation of dye waste water.
Accompanying drawing explanation
Fig. 1 is samarium doping KMgF of the present invention3The process chart of Ca-Ti ore type visible light response catalyst preparation method;
Fig. 2 is samarium doping KMgF of the present invention3Ca-Ti ore type visible light response catalyst KMgF front with doping3The perovskite type catalyst degradation effect comparison diagram to rhodamine B.
Detailed description of the invention
Below in conjunction with drawings and Examples, technical scheme is described in detail.
Embodiment 1
Samarium doping KMgF of the present invention3The preparation method of Ca-Ti ore type visible light response catalyst, comprises the steps:
Step 1, adds 13.4146g cetyl trimethylammonium bromide [CTAB] in 80.4876g isooctanol [2-EH], stirs 2h, be configured to solution A under room temperature; By 0.2022g (0.002mol) potassium nitrate [KNO3], 0.5128g (0.002mol) magnesium nitrate hexahydrate [Mg (NO3)2��6H2O], 0.0089g (0.00002mol) six nitric hydrate samarium [Sm (NO3)3��6H2O] add in 7ml deionized water, stir 5min, be configured to solution B; By 0.2222g (0.006mol) ammonium fluoride [NH4F] add in 3ml deionized water, stir 5min, be configured to solution C; Under constant agitation, successively solution B and solution C are added dropwise in solution A, form the microemulsion of homogeneous transparent continuously stirred 1h again;
Step 2, the microemulsion centrifugation that step 1 is obtained, the speed of centrifugation is 4000r/min, and the time is 15min; The precipitation methanol (analytical pure) obtained after centrifugal is washed 5 times, dry 24h under room temperature;
Step 3, desciccate step 2 obtained is placed in tube furnace, in nitrogen atmosphere, rises to 400 DEG C with the speed of 10 DEG C/min, and calcines 30min at 400 DEG C, naturally cools to room temperature, namely obtains samarium doping KMgF3Ca-Ti ore type visible light response catalyst KMgF3��Sm��
Embodiment 2
Samarium doping KMgF of the present invention3The preparation method of Ca-Ti ore type visible light response catalyst, comprises the steps:
Step 1, adds 13.4146g cetyl trimethylammonium bromide [CTAB] in 80.4876g isooctanol [2-EH], stirs 2h, be configured to solution A under room temperature; By 0.2022g (0.002mol) potassium nitrate [KNO3], 0.5128g (0.002mol) magnesium nitrate hexahydrate [Mg (NO3)2��6H2O], 0.00004mol six nitric hydrate samarium [Sm (NO3)3��6H2O] add in 7ml deionized water, stir 5min, be configured to solution B; By 0.2222g (0.006mol) ammonium fluoride [NH4F] add in 3ml deionized water, stir 5min, be configured to solution C; Under constant agitation, successively solution B and solution C are added dropwise in solution A, form the microemulsion of homogeneous transparent continuously stirred 1h again;
Step 2, the microemulsion centrifugation that step 1 is obtained, the speed of centrifugation is 4000r/min, and the time is 15min; The precipitation methanol (analytical pure) obtained after centrifugal is washed 5 times, dry 24h under room temperature;
Step 3, desciccate step 2 obtained is placed in tube furnace, in nitrogen atmosphere, rises to 400 DEG C with the speed of 10 DEG C/min, and calcines 30min at 400 DEG C, naturally cools to room temperature, namely obtains samarium doping KMgF3Ca-Ti ore type visible light response catalyst KMgF3��Sm��
Embodiment 3
Samarium doping KMgF of the present invention3The preparation method of Ca-Ti ore type visible light response catalyst, comprises the steps:
Step 1, adds 13.4146g cetyl trimethylammonium bromide [CTAB] in 80.4876g isooctanol [2-EH], stirs 2h, be configured to solution A under room temperature;By 0.2022g (0.002mol) potassium nitrate [KNO3], 0.5128g (0.002mol) magnesium nitrate hexahydrate [Mg (NO3)2��6H2O], 0.0267g (0.00006mol) six nitric hydrate samarium [Sm (NO3)3��6H2O] add in 7ml deionized water, stir 5min, be configured to solution B; By 0.2222g (0.006mol) ammonium fluoride [NH4F] add in 3ml deionized water, stir 5min, be configured to solution C; Under constant agitation, successively solution B and solution C are added dropwise in solution A, form the microemulsion of homogeneous transparent continuously stirred 1h again;
Step 2, the microemulsion centrifugation that step 1 is obtained, the speed of centrifugation is 4000r/min, and the time is 15min; The precipitation methanol (analytical pure) obtained after centrifugal is washed 5 times, dry 24h under room temperature;
Step 3, desciccate step 2 obtained is placed in tube furnace, in nitrogen atmosphere, rises to 400 DEG C with the speed of 10 DEG C/min, and calcines 30min at 400 DEG C, naturally cools to room temperature, namely obtains samarium doping KMgF3Ca-Ti ore type visible light response catalyst KMgF3��Sm��
Measure the KMgF of embodiment 1��3 preparation respectively3��Sm3+To the visible light photocatalytic degradation ability of rhodamine B molecule in solution:
Taking 100mL rhodamine B initial concentration is the solution of 20mg/L, adds the KMgF of 0.1g embodiment 1 preparation3: Sm photocatalyst, constant temperature oscillation 30min, upon adsorption reach balance after, open visible light source irradiate 2h, carry out visible light catalytic reduction experiment, in experiment, sample 2ml, centrifugation every 10min, taking supernatant, measure absorbance by ultraviolet-uisible spectrophotometer, result is as shown in table 1;
Taking 100mL rhodamine B initial concentration is the solution of 20mg/L, adds the KMgF of 0.1g embodiment 2 preparation3: Sm photocatalyst, constant temperature oscillation 30min, upon adsorption reach balance after, open visible light source irradiate 2h, carry out visible light catalytic reduction experiment, in experiment, sample 2ml, centrifugation every 10min, taking supernatant, measure absorbance by ultraviolet-uisible spectrophotometer, result is as shown in table 1;
Taking 100mL rhodamine B initial concentration is the solution of 20mg/L, adds the KMgF of 0.1g embodiment 3 preparation3: Sm photocatalyst, constant temperature oscillation 30min, upon adsorption reach balance after, open visible light source irradiate 2h, carry out visible light catalytic reduction experiment, in experiment, sample 2ml, centrifugation every 10min, taking supernatant, measure absorbance by ultraviolet-uisible spectrophotometer, result is as shown in table 1;
Table 1
| Selected materials | Rhodamine B residual concentration (mg/L) in solution | Clearance (%) |
| Catalyst in embodiment 1 | 1.54 | 92.3 |
| Catalyst in embodiment 2 | 0.4 | 96 |
| Catalyst in embodiment 3 | 1.28 | 93.6 |
��
KMgF to embodiment 2 preparation3: the KMgF before Sm photocatalyst and samarium doping3Photocatalyst carries out rhodamine B visible light photocatalytic degradation experiment:
Taking two parts of 100mL rhodamine B initial concentrations respectively is the solution of 20mg/L, adds the KMgF of 0.1g embodiment 2 preparation in a copy of it rhodamine B solution3: Sm photocatalyst, another part of rhodamine B solution adds the KMgF before 0.1g samarium doping3Photocatalyst, constant temperature oscillation 30min, upon adsorption reach balance after, open visible light source irradiate 2h, carry out visible light catalytic reduction experiment. In experiment, sampling 2ml, centrifugation every 10min, take supernatant, measure absorbance by ultraviolet-uisible spectrophotometer, result is as shown in Figure 2.
Figure it is seen that the catalyst before samarium doping compared by the catalyst after samarium doping, under visible light conditions, catalytic effect has had and has been substantially improved, and illustrates that samarium doping can be substantially improved the catalyst utilization rate for visible ray.
Obviously, above-described embodiment is only for clearly demonstrating example of the present invention, and is not the restriction to embodiments of the present invention. For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description. Here without also cannot all of embodiment be given exhaustive. And the apparent change that these spirit belonging to the present invention are extended out or variation are still among protection scope of the present invention.
Claims (6)
1. a samarium doping KMgF3Ca-Ti ore type visible light response catalyst, it is characterised in that: for every 1molKMgF3, Sm3+The doping of ion is 0.01��0.03mol, Sm3+Ion doping is in B bit element Mg2+On ion.
2. samarium doping KMgF described in a claim 13The preparation method of Ca-Ti ore type visible light response catalyst, it is characterised in that: comprise the steps:
Step 1, adds a certain amount of cetyl trimethylammonium bromide in isooctanol, is configured to solution A after mixing; A certain amount of potassium nitrate, magnesium nitrate hexahydrate and six nitric hydrate samariums are added to the water, are configured to solution B; A certain amount of ammonium fluoride is added to the water, is configured to solution C; Under constant agitation, successively solution B and solution C are added dropwise in solution A, form the microemulsion of homogeneous transparent continuously stirred a period of time;
Step 2, the microemulsion centrifugation that step 1 is obtained, undertaken the precipitation after centrifugal washing, dried;
Step 3, calcines the product of step 2 in nitrogen atmosphere, namely obtains samarium doping KMgF after calcining cooling3Ca-Ti ore type visible light response catalyst.
3. samarium doping KMgF according to claim 23The preparation method of Ca-Ti ore type visible light response catalyst, it is characterised in that: in step 1, in solution A, the addition mass ratio of described cetyl trimethylammonium bromide and isooctanol is 1: 6.
4. samarium doping KMgF according to claim 23The preparation method of Ca-Ti ore type visible light response catalyst, it is characterised in that: in step 1, in described microemulsion, the addition mol ratio of potassium nitrate, magnesium nitrate hexahydrate, six nitric hydrate samarium potassium nitrate and ammonium fluoride is 1: 1: 0.01��0.03: 3.
5. samarium doping KMgF according to claim 23The preparation method of Ca-Ti ore type visible light response catalyst, it is characterised in that: in step 2, the speed of described centrifugation is 4000r/min, and the time is 15min; The cleaning mixture that described washing adopts is methanol.
6. samarium doping KMgF according to claim 23The preparation method of Ca-Ti ore type visible light response catalyst, it is characterised in that: in step 3, the temperature of described calcining is 400 DEG C, and described calcination process is to be risen to 400 DEG C by room temperature, and its heating rate is: 10 DEG C/min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106669749A (en) * | 2016-06-28 | 2017-05-17 | 河海大学 | Fe-doped KMgF3 perovskite type visible-light response catalyst and preparation method thereof |
| CN106669748A (en) * | 2016-06-28 | 2017-05-17 | 河海大学 | Iron-doped NaMgF3 perovskite type visible light response catalyst and preparation method thereof |
| CN107487787A (en) * | 2017-10-12 | 2017-12-19 | 北京科技大学 | A kind of hollow KMnF3The preparation method of nanometer square particle |
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| CN1342598A (en) * | 2001-10-12 | 2002-04-03 | 中国科学院长春应用化学研究所 | Process for synthesizing low-oxygen perovskite-type compound fluoride |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106669749A (en) * | 2016-06-28 | 2017-05-17 | 河海大学 | Fe-doped KMgF3 perovskite type visible-light response catalyst and preparation method thereof |
| CN106669748A (en) * | 2016-06-28 | 2017-05-17 | 河海大学 | Iron-doped NaMgF3 perovskite type visible light response catalyst and preparation method thereof |
| CN106669749B (en) * | 2016-06-28 | 2019-12-10 | 河海大学 | Iron-doped KMgF 3 perovskite type visible light response catalyst and preparation method thereof |
| CN107487787A (en) * | 2017-10-12 | 2017-12-19 | 北京科技大学 | A kind of hollow KMnF3The preparation method of nanometer square particle |
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